Innovations in ICP Sample Introduction Jerry Dulude Glass

Innovations in ICP Sample Introduction Jerry Dulude, Glass Expansion, Inc. 4 Barlows Landing Rd. Pocasset, MA Glass Expansion

Summary of Discussion n Low Flow Nebulizers n Helix O’ring-free Spray Chambers n New Internal Standard Kit n Niagara Rapid Rinse Accessory Glass Expansion Innovations in Sample Introduction

Applications of Low-Flow Nebulizers n Limited sample volumes n Volatile samples n Expensive waste disposal n ICP-MS-LC interface Glass Expansion Low-Flow Nebulizers

Range of Low-Flow Nebulizers n Micro. Mist- Concentric glass nebulizer n 0. 05 to 0. 6 ml/min n Poly. Con- Concentric polyimide nebulizer n 0. 05 to 0. 6 ml/min n Opal. Mist- Concentric PFA nebulizer n 0. 01 to 0. 6 ml/min Glass Expansion Low-Flow Nebulizers

Transport Efficiency vs. Uptake %EFFICIENCY UPTAKE RATE (ML/MIN) Indirect drain collection method Glass Expansion Low-Flow Nebulizers

Tertiary Flow Rate vs. Uptake Tertiary Flow Rate (ul/min) Glass Expansion Low-Flow Nebulizers

Corroboration of Tertiary Flow Rates Uptake rate (ml/min) Indirect Method (mg/min) Direct Method* (mg/min) 0. 03 15 14 0. 11 23 21 v. Todoli, Hernandis, Canals, and Mermet, JAAS, 1999, 14, 1289 -1295 Using GE Micro. Mist nebulizer with U-tube absorption for measurement Glass Expansion Low-Flow Nebulizers

Primary Aerosol Size Distribution Comparison Nebulizer Gas Flow Rate = 1. 0 L/Min Solution Uptake Rate = Natural Aspiration Conikal (2 ml/min) 100 D 32 = 17. 2 60 Normalized Volume Normalized Count 20 Micro. Mist (0. 03 ml/min) 100 D 32 = 7. 1 60 20 0 10 20 30 Diameter (mm) Glass Expansion 40 50 60 0 10 20 30 40 Diameter (mm) Low-Flow Nebulizers 50 60

Tertiary Aerosol Size Distribution Comparison Nebulizer Gas Flow Rate = 1. 0 L/Min Solution Uptake Rate = Natural Aspiration Baffled Cyclonic Spray Chamber Conikal (2 ml/min) 100 D 32 = 4. 9 Normalized Count 60 20 Micro. Mist (0. 03 ml/min) 100 D 32 = 5. 0 60 20 0 10 20 30 40 50 Diameter (mm) Glass Expansion Low-Flow Nebulizers

New Micro-Flow Opal. Mist n All PFA construction n Natural uptake rate of 0. 010 ml/min n Ultra-high purity applications n Ideal for micro samples down to 20 ul volume Glass Expansion Low-Flow Nebulizers

Cyclonic Spray Chambers Advances in Nebulizer Installation 1993 1984 1996 Glass Expansion Helix O’ring free spray chamber

Helix O'ring-Free Spray Chamber n Reduced carryover n Faster washout n Higher purity n Can stand up to ketones and other solvents Glass Expansion Helix O’ring free spray chamber

New Internal Standard Kit Benefits of Internal Standardization n Compensate for physical interferences n Viscosity n Surface tension n Compensate for some chemical interferences n High salts n Mass related effects (ICP-MS) n Improve short term precision (simultaneous detectors) n Decrease long-term drift Glass Expansion Internal Standard Kit

New Modular Internal Standard Kit Glass Expansion Internal Standard Kit

IS Tee with Built-in Mixing Chamber Glass Expansion Internal Standard Kit

New Flared-End Pump Tubing The final building block of a totally modular system Glass Expansion Internal Standard Kit

IS Schematic Peri Pump Sample Glass Expansion IS Internal Standard Kit

Niagara™ Rapid Rinse Accessory n Interfaces between ICP & Autosampler n Reduces required rinse time n Programmable delay time n Less than 8 inches high n Includes adj. height stand Glass Expansion Rapid Rinse Accessory

How Niagara Works Analysis Glass Expansion Rinse Rapid Rinse Accessory

Niagara Time Saving (30 sec rinse) Standard System With Niagara Probe to sample 5 5 Uptake delay 15 15 Stabilization 10 10 Read 15 15 Probe to rinse 5 5 Rinse 30 5 Total (seconds) 80 55 = Rinse steps Glass Expansion Rapid Rinse Accessory

Summary n Micro. Mist nebulizers n Efficient sample consumption n Minimum waste generation n Helix spray chambers n Eliminate o’ring maintenance and contamination n Reduce carryover n Internal standard kit n Improved accuracy without the work n Easy & inexpensive modular replacement n Niagara Rapid Rinse Accessory n More samples per hour n Faster sample turnaround time Glass Expansion Rapid Rinse Accessory